Apparatus for extracting albumins from plants.



J. GEISTDURPER. APPARATUS FOR EXTRACTING ALBUMINS FROM PLANTS. APPLICATION FILED DEC. 24, 1909.

2 BHEETS-SHEET 1.

WITNESSES J. GEISTD O RPER. APPARATUS FOR EXTRAGTING ALBUMINS PROM PLANTS.

APPLICATION FILED DBO. 24, 1909. 1,003,594.

gzilvrofi M4 ATTORNEYS.

Patented Sept. 19, 1911.

- 2 SHEETS-SHEET 2. 1 Q

JEA snxs'rnonrnza, or rams, FRANCE.

APPARATUS FOR EXTRACT ING ALBUMINS FROM PLANTS.

incense.

Specification of Letters Patent.

Patented Sept. 19, 1911.

Application filed December 24, 1909. Serial No. 534,795.

terial in question with alcohol heated to 50 to 90 C. The albumin is then precipitated from the alcoholic solution with ether, absolute alcohol, excess of water or dilute acids.

Technically the production offers great dif-- ficulties, firstly, with regard to the recovery of the alcohol, and, secondly, with regard to obtaining a precipitate which can be readily collected, washed, dried and purified containing no alcohol, and not agglomerating into a sticky mass.

having a vertical axis.

An important ob ect of my invention is to provide a commercial process for obtaining from vegetable matter albumin soluble in alcohol and in the form of a solid mass.

My process completely overcomes the above mentioned difficulties and comprises 'two principal operations :'Firstly, the extraction of the albumin by means of hot alcohol with the aid of a vacuum which assures-complete lixiviation and almost complete recovery of the alcohol, and excludes all danger of fire; secondly, the precipitation of the albumin while in motion, not alone withthe aid of water, ether, absolute alcohol and-dilute acids, as is already known, but also with other than the mentioned recipitants, such as glycerin, oils, tetrachlorid of carbon, turpentine, with or Without the admixture of strong acids, or other suitable liquids.

My process necessitates the employment of two apparatuses, firstly a lixiviating device working with the aid of a vacuum, and secondly a precipitating pan for precipitation in motion provided with an a itator The centri aging, drying and disintegration have nothing peculiar about them or are well-known operations and are not further described herein.

As starting materials I may em loy the most various disintegrated or groun cereals,

as, e. g. barley, maize, wheat, rice, man'ick,

soja, and so on; also, the various legumes; further, commercial residues of albiminous materials from malt houses and breweries, starch, glucose and, dextrin works; waste from rice, flour, bran, and so on; lastly,'in addition, oil cake, earth nuts, and so on.

In order that my invention may be clearl understood I will now explain the same with reference .to the accompanying drawing in which apparatus suitable for carrying my process nto practice is represented by way of example.

In said drawing: Figures 1 and 1 are diagrammatic elevations, partly in section, and Fig.2 is a detail. r

Referring to the'drawing, the lixiviating apparatus comprises a plurality of individual leaching-vats, of which three are represented and designated a, a anda but the number may be optional. Each of these vats has a removable lid 1 normally closed airtight, an air-inlet cock2 and a thermometer 3. In addition each vat has a water-gage, not shown in the drawing, admitting of the level 4 of the liquid within being and also a discharge cock 5 for withdrawing tests. The lids are secured by hinged screws, not shown, a packing of caoutchouc or other suitable material, also not shown, being laced under them. In each vat is a sheetron, cylinder or drum 6 having a perforated bottom covered with a sieve, in which is located the substance to be lixiviated. Each drum rests on a circular angle-iron 7 riveted to the Wall of'thc vat. Each drum has two handles 8, as shown in Fig. 2, allowing them to be handled more easily. The walls of the vats maybe doubled for heating the mass which is to be lixiviated by passing steam between the same.

observed,

9 designates a common alcohol vapor pipe connected with the vats by pipes 10, 11 and 12 having cocks 13,

16 is a shut-ofi cock. 17 is a common steam pipe connected with the vats by pipes 18, 19 and 20 having cocks 21, 22 and 23, respectivel 1 24 designates a shut-o cock.

14 and 15, respectively.

' 35 cock 74.

v cylinder presses not shown in is a "common. vacuum pipe connected with the vats by pipes 26, 27 and 28Jhaving cocks 29, 30 and 31, respectively.

32 designates a shut-ofi cock.

33 is a common alcohol pipe connected with the vats by pipes 34, 35 and 36 having cocks 37 38 and 39, respectively; 40 and 41 designate shut-ofi' cocks; 42, 43 and 44 are cocks which regulatethe circulation b tween 1@ the vats. Said pipes. 34, 35 and 36 re incased with a jacket 45into which steam may be passed for heating the alcohol.

46' designates a common condensed-water pipe with which the vats are connected by 5 pipes 47, 48 and 49 having Q'QCRSQQ, 1 and 52, respectively. 7

. 53 designates a shut-ofi' cock.

7 54 is a common vacuumpipe corresponding to the pipe 25'which works just like this 0 and is connected with the vats by pipes 55,

56 and 57 having cocks 58, 59 and '60, respectively. Said' pipe 54 is optional. The vats are interconnected by "pipes 62, 63 and 64 having cocks 65, 66 and 67, respectively.

b designates a vacuum receiver or pan having a manometer 68 and an air-inlet cook 69. In open relation with this pan is a pipe 70 having a shut-off cock-71.. In 30 addition said pan has a water-gage-not represented in the drawing. .By means-of the discharge cook 72 the liquid can be run from pen I) into the cooler c and storage-tank at having air-admission cock 73 and bib.-

e designates a pan for precipitation while the liquid'is in motion having a vertical axle 75. Agitatingarms' 76 are secured-onfihe bross arm 77 secured to axle 7 5..

.. 49 v 78 designates a shut-off cock in the pipe connecting pan e with the centrifuges or t 6 drawing. f designates a suction tank condensed Water havin an air-inlet cook '79 and a, discharge 000 80.

82 is a suction pipe havingcock 83. A

water-gage, notshown, admits of the height of the liquid in tank f being observed. (The pan 6 cannot be used here as the condensed .waterwould precipitate the albumin'which .would stop up the pipes.)

84 designates a tank fwith the condenser 9.

- alcohol.

86 designates .a'shut-ofi' cock and 87 an air-inlet cock.

90 designates a suction p'pe connecting the washing tower j with receiver 72.. 91 1s a shut-off cock in'the latter pipe.

- 61 designates a "shut-ofl' cock.

- the alcohol circulates,

for steam and r 71, 83,32, 29,30, 31 are opened and pipe connecting pan band p dlcates a pressure 85 designates a pipe connecting condenserg with the receiver or tank h for condensed 88 is a manometer and 89 a discharge cock.

92 is a suction p pe leading to the m designates a common vacuum receiver connected with the vacuum pump by pipe 95 having the cock 96 and with suction pipe 92 by way of cook 97. This receiver has .a Vacuum gage 98.

99 is an inlet cock for admitting hot air or steam, and 100 is a. discharge cock.-

101 is a discharge pipe and n a pan or cistern connected with the Washing tower p by pipe 102. The towers j and p are alike and comprise individual plates j provided ways remains on these plates at a definite height and the alcohol vapors which are sucked in or are returning are condensed in it.

103 designates a hopper having 'a shutofi cock 104. 105 designates a bib-cock and 106 adpipe for discharging non-condensed gases an vaors. p The principle on which my a paratus operates is as follows:-The alcohol which is charged most completely with albumins is brought together with the substance richest in albumin, 2'. e. that freshly charged in, and the alcohol charged leas wlth albumins with the substance most lixiviated. The liquid of each individual extraction passes onrby .itself separately in such manner that, before :is sent from one vat into the next, the alcohol which is in this latter vat is allowed to flow into the following one. In addition, when passing through each individual vat, through the mass to be lixiviated in succession from below upward and from above downward. This has the advant-age, as compared with the diffusion process, that the lixiviation is better and more ra id and a more'concentrated ,solution .is o tained. The, emloyment of a vacuum prevents the alcohol vapors spreading in the space or chamber in question and thus removes all danger of fire.

Referring now to the drawing, after the yats or extractors a, a; and a have been charged andall the cooks have 'beenclosed,

a vacuum is produced in the entire apparatus. For this purpose cocks 96, 97 91, 86,

When the manometer inbelow atmospheric of 650 to 700'mm. mercury, cocks.83 and 96 are closed and cook 94 is opened. The pump may then be stopped. Then cocks'29,- 30 and 31 are closed a am. W hen the condenser is cooled and t e alcohol heated tothe required temperature, the alcohol is allowed to enter into extractor a by opening cocks 41,42, 43 and 44 and finally 37.

Under the influence of the vacuum alcohol flows through pipe v33and rises in pipe 34.-

K is set working.

When thelevel 4 is reached cocks 37, 4 2, 43, 44 and 41 areclosed and the/apparatus is with overflows 7' Consequently water al-' ..the alcohol or the alcoholic albumin solution left alonefor five or ten minutes. When working normally, during this time the alcohol charged with-albumin is allowed'to pass from vat a into vat a and a vacuum is pro- 5 duced in that extractor which is'freshly charged or in suction tank f and receiver m. The alcohol char ed with albumins is then allowed to ass rom vat a into vat a by openin r coc s 40, 42, 38 and 66. By opening co e (s 16 and 13, alcohol vapors ilfre simultaneously allowedto enter into ex 'actor a so that the vacuum produced ,thereimdoes not prevent the discharge. This alcohol vapor simultaneously heats the solvent alcohol. Instead of doing this, however, .cock 29 may be opened in order to. equalize the pressure below and above in the extractor, orairinlet cock 2 may be opened. The alcoholic extract from extractor aasses through pipe 63 to extractor a and w en the level in extractor a has sunk one half, coc'ks66, 40, 42, 16 and 13 are closed. The mass contained in extractor a is now saturated with alcohol and the alcoholic albumin-solution has not yet been able to enter into the pipe 33; then alcohol is allowed to pass from extractor a to extractor a in the reverse direction without the aid of pipe 63, by opening in succession cocks 32, 30, 38, 42, 37 and subsetquently cocks 16 and. 13. The albumin so-- lution which remained in extractor 0. passes through pipes 34, 33, and rises into extractor a Simultaneously alcohol vapor flows through pipes 9 and 10 into extractor a, then through the mass saturated with alcohol in extractor a and partially condenses there and heats the same. The vapor not condensed in extractor 0.- passes to the condenser g through pipes 27 and 25,

vacuum receiver 1), ipes 70 and 84, and the condensed alcohol ows thenc into tank h, from which it is drawn off fro time to time to supply it again to the system. The alcohol vapors not retained b pass to tower j which retalns them, but in the event of traces of alcohol passing thence they are stopped by tower In order to heat the alcohol circulating f r-om, extractora to extractor a} steam is referably assed around pipes 34 and 35. hen the a cohol flows away only badly from the mass con tained in extractor a, cocks 16 and 13 are closed and air-inlet cock '2 of extractor a is opened, while the pump constantly sucks away as much alcoholas possible from, extractor a. When the level 4 has been reached in extractor a and when-extractor a contains hardly any liquid, cocks 30, 2, 38, 42 and '37 are closed. Instead of pipe 25 pipe 54 may be used or both jointly. The mass in extractor a is not yet fully lixiviated. Consequently alcohol is afresh sent e into the extractor in the manner above described. The solution which is noticeably 65 concentrated with albumins ,is allowed then I iviated.

the condenser.

' may be considered lixiviated, it is emptied,

necessary as the vacuum can to pass from extractor a to extractor a? and, lastly, that from extractor a to extractor a, as above described. The material contained in extractor a may then be considered as lix This can be determined by takin a test from extractor a by means of cocc' 5 and then precipitating with acidified water. In order to expel the alcohol contained in the mass in extractor a, a current of hot air or steam is sent through cocks 53, 50,.24 I and 21, the other cocks remaining closed. The alcohol or alcohol-water vapors condense in suction tank 7 where the vacuum is produced. Vacuum tank 6 cannot be employed for this as the water would precipitate the albumins .which might cause the pipes to be stopped up.

The liquid condensed in tank f is discharged, before a fresh vacuum is produced, by closing cocks71, 8G and opening cocks 79, 80. The diluted alcohol 1s conducted into a common tank or collector for weak alcohol, into which are sent, in addition, the

liquids discharged by the centrifuges or presses. This alcohol is subsequently concentrated by distillation and returned to the system. In this manner almost the entire alcohol is recoyered w 'ch saturated the mass to be lixiviated and which cannot be recovered solely by suction.

'95 Cocks 53, 50, 24, 21 are then closed and "then lid 1 is removed from extractor a, the

drum 6 is emptied, charged afresh, remserted and the lid secured. Then a vacuum is produced in extractor a as previously described. In extractor a the albumm solution .is sufliciently concentrated. It is drawn off by opening cocks 40, 39 and the air-inlet cock 2 of extractor (H. The liquid flows away through pipes 36, 33 into vacuum pan 1). The same is sent into'tank d by closing cocks 40, 71 and opening cocks 69, 72, 73. The apparatus is then working normally, 2'. 6. when extractor a is two-thirds lixivi. ated, extractor a one-third and extractor a vcharged with fresh raw material. Then ure alcohol is sent into extractor a, thence mto extractor a. and finally into extractor 'a, whence it is drawn oil. When extractor a charged afresh, evacuated, and so on. The cycle ofoperations remains the same however large the number of extractors may be. The mode of operation of towers j and p does not require to be more particularly ex plained; they may be substituted by any other suitable system. In the event of alcohol condensing in receiver m, a current of hot air or steam is sentthrough cook 99, and the condensed liquid is collected in the collector, not represented in the drawing, for weak alcohol together with the diluted alcohol coming from the tank f.

The vacuum receiver m' is not absolutely be mroducfi 130 without its aid by closing cocks 96 and 97 and opening'93. But as it has a large ca pacity it enables the vacuum to be maintained without the pump working continuously. For this purpose a. vacuum is produced in receiver m by closing cocks 9.7, 93 and opening cock 96. When the vacuum 740 mm. of mercury is obtained, cock 96 is closed and the pump is stopped. In the event of the pressure in the a paratus having to be increased, it is su cient to open cock 97 to again bring about the normal operating pressure in the apparatus. Receiver -m can 'be subsequently evacuated afresh and operations may proceed in like manner. i

In order toproduce a vacuum in a freshlycharged extractor it is advantageous'to produce the vacuum directly by cutting out receiver m and opening cook 93. Receiver m is, however, a convenient auxiliary for rapidly equalizing a small admission of air without starting the pump. 1' As the two described modes of operation are independent of one another, they may be employed simultaneously. 7 a The condensation of the alcohol vapor in .condenser 9 produces in itself a certain vacuum, and consequentlythe apparatus can work for a certain time with this condensation without the pressure rising. It suffices to close cock 91 and observe manometer 88. When large quantities of air enter the apparatus, the vacuum must of course be produced by the pump.

The albumin solution contained in vacuum pan 6 passes into cooler cwhich cools it, and then into tank 03. When the precipitation pan e is filled to a certain height, exactly indicated by' a mark on the wall, with as much water or other suitable liquid, such as dilute acids, glycerin or the like,,as is necessary for precipitating a definite volume of the albumin so ution, the agitator is set working. Cocks 73 and 74 are then opened quite gradually in order to allow the albumin solution to flow into the liquid contained in pan e up to a second marked point which indicates the volume which can be precipitated by the liquid contained injthe precipitation pan. Under these conditions the albumins are obtained as firm flakes, and notas a. viscous mass, which do not a tain little alcoho1. He the agitator remains in motion, cocks 73 and 74 are closed and cock 78 is ,opened. The liquid passes thence directly into the centrifuges or into the filter presses. I It may, however, be collected in a tank and allowed to stand. a After to minutes the precipitated albumin settles, so that it can be readily separated from the liquid over it.; It is liberated in optional manner from the adhering liquid and then it has only to be dried, pulverized, and so on. Theprecipt glomerateand con- The albumin solution may also be precipi-' tated as follows: Insteadof precipitating the albumins by agitation in water, as described above, I may simply dilute the alcohol and place the solution in a vacuum, the

alcohol vapors being sucked off by vacuum and condensed. By this process the alcohol is completely recovered on the one hand, and

ghe, product is obtained dry on the other My improved process and the hereindescribed apparatus may serve, without material modification, for the extraction of albumins which are insoluble in alkalis but soluble in weak alkaline lyes, and also for lixiviating all other;substances b means ofoptional solvents, for example or the lixiviation of bark for the purpose of manufacturing tannin extract, for the extraction of fatty substances by means of tetrachlorid of carbon, and the like.

It is to be understood that the details of the hereindescribed mode of operation as well as the construction of the apparatus may be modified within certain limits without departing from the spirit and scope of my invention.

I claim: a

1. In extractingapparatus of the character described, the combination, with a plu: rality of vats, of pipes, each provided with a cock, interconnecting said vats one with another, ,a vacuum tank, a common vacuum pipe connected with said tank, pipes, each having a cock, connecting said vacuum pipe with the upper portions of said vats, a common circulation pipe, 'havin a cock, connected with said tank, and pipes, each having a cock, connectingsaid circulation pipe with the lower portions of said vats; a. common alcohol-vapor pipe having a cock, and

pipes, each having a cock, connecting said alcohol-vapor pipe with the to portions of said vat-s3 a second suction tanr; and pipes .each having a cock, connecting said secon tank with the bottom-portions of said vats, for the purpose specified.

'2. In extracting apparatus of thecharacter described, the combination, with a plurality of vats, of pipes, each provided with a; cock, interoonnectm said vats one with another, a vacuum taxi, a common vacuum pipe connected with saidtank, pipes, each having a cock, connecting said vacuum pipe with the upper portions of said vats, a' common circu ation. pipe, having a cock, connected with said tank, andpipes, each having a cock, connecting said circulation pipe tank with the bottom portions of said vats, 10 with the lower portions of said vats; a comfor the purpose specified.

mon alcohol-vapor pipe having a cock, and In testimony whereof, I afliX my signature pipes, each having a cock, connecting said in the presence of the Witnesses.

alcohol-vapor pipe with the top portions of I JEAN GEISTDORFER. said vats; a second suction tank; pipes, each Witnesses:

having a cock, connecting the top portions DEAN B. MASON.

of said vats With said second tank, and pipes, FRED. GRAFTON,

each having a cock, connecting said second -ERNEST MOHR. 

